close

Вход

Забыли?

вход по аккаунту

?

Crystallographic report Dimeric tetraphenyl-1-hydroxo-3-trifluoromethanesulfonatodistannoxane [Ph2(HO)SnOSn(O3SCF3)Ph2]2.

код для вставкиСкачать
APPLIED ORGANOMETALLIC CHEMISTRY
Appl. Organometal. Chem. 2004; 18: 51–52
Main
Published online in Wiley InterScience (www.interscience.wiley.com). DOI:10.1002/aoc.562
Group Metal Compounds
Crystallographic report
Dimeric tetraphenyl-1-hydroxo-3trifluoromethanesulfonatodistannoxane,
[Ph2(HO)SnOSn(O3SCF3)Ph2]2
Jens Beckmann*, Dainis Dakternieks, Andrew Duthie and Cassandra Mitchell
Centre for Chiral and Molecular Technologies, Deakin University, Geelong 3217, Australia
Received 9 September 2003; Revised 16 September 2003; Accepted 17 September 2003
The molecular structure of the title compound, obtained by an adventitious phenyl
group cleavage of Ph3 SnOSnPh3 with triflic acid, reveals discrete centrosymmetric units of
[Ph2 (HO)SnOSn(O3 SCF3 )Ph2 ]2 that are loosely associated via hydrogen bonding. Copyright  2004
John Wiley & Sons, Ltd.
KEYWORDS: crystal structure; tetraorganodistannoxane; tin
COMMENT
*Correspondence to: Jens Beckmann, Centre for Chiral and Molecular
Technologies, Deakin University, Geelong 3217, Australia.
E-mail: beckmann@deakin.edu.au
Contract/grant sponsor: Deakin University.
Contract/grant sponsor: Australian Research Council.
Several crystals of [Ph2 (HO)SnOSn(O3 SCF3 )Ph2 ]2 were
isolated from the reaction of an equimolar ratio of
Ph3 SnOSnPh3 and triflic acid, with the intention of
Figure 1. Molecular structure of [Ph2 (HO)SnOSn(O3 SCF3 )Ph2 ]2 . Hydrogen atoms attached to carbon atoms are omitted for
clarity. Selected geometric parameters: Sn1–O1 2.117(3), Sn1–O1i 2.064(3), Sn1–O2i 2.177(4), Sn1–C11 2.109(5), Sn1–C21
2.091(6), Sn2–O1 2.017(3), Sn2–O2 2.093(4), Sn2 –O3 2.306(3), Sn2–C31 2.121(5), Sn2–C41 2.112(5) Å; O1–Sn1–O1i 73.97(13),
O1–Sn1–O2i 146.98(13), O1–Sn1–C11 99.61(18), O1–Sn1–C21 98.7(2), O1i –Sn1–O2i 73.20(13), O1i –Sn1–C11 113.21(17),
O1i –Sn1–C21 115.99(20), O2i –Sn1–C11 96.38(18), O2i –Sn1–C21 92.41(19), C11–Sn1–C21 130.5(2), O1–Sn2–O2 75.95(14),
O1–Sn2–O3 80.40(14), O1–Sn2–C31 111.00(17), O1–Sn2–C41 117.62(18), O2–Sn2–O3 156.17(14), O2–Sn2–C31 98.57(19),
O2–Sn2–C41 95.33(19), O3–Sn2–C31 92.49(18), O3–Sn2–C41 93.04(19), C31–Sn2–C41 131.3(2)◦ . Hydrogen bonding contact:
O2· · ·O4ii 2.806(6) Å. Symmetry operations: i, 2 − x, −y, 2 − z; ii, 1.5 − x, −0.5 + y, 1.5 − z.
Copyright  2004 John Wiley & Sons, Ltd.
52
J. Beckmann et al.
producing [Ph3 SnOHSnPh3 ](O3 SCF3 ). The formation of
[Ph2 (HO)SnOSn(O3 SCF3 )Ph2 ]2 (Fig. 1) may be rationalized
by an adventitious phenyl group cleavage similar to that
reported recently for the reaction of Ph3 SnOSnPh3 with
2,4,6-tris(trifluoromethyl)benzoic acid.1 The title compound
is an analogue of [R2 (HO)SnOSn(O3 SCF3 )R2 ]2 (R = Et, nBu, n-Oct),2 and an example of the broader class of dimeric
tetraorganodistannoxanes.3
Main Group Metal Compounds
1455.72, monoclinic, P21 /n, a = 11.4025(7), b = 16.3884(10), c =
15.3933(9) Å, β = 110.285(1)◦ , V = 2698.1(3), Z = 2, 6127 unique
data (θmax = 27.5◦ ), R = 0.046 (4259 [I > 2σ (I)] reflections), wR =
−3
0.109 (all data), ρmax = 1.18 e−1 Å
(near tin). Programs used:
SAINT, SADABS, SHELX-97, ORTEP. CCDC deposition number:
218 184.
Acknowledgements
The Australian Research Council (ARC) is thanked for financial
support. Dr Jonathan White (The University of Melbourne) is
gratefully acknowledged for the data collection.
EXPERIMENTAL
Triflic acid (0.204 g, 1.36 mmol) was added to Ph3 SnOH
(1.00 g, 2.72 mmol) suspended in MeCN (50 ml) and stirred
at room temperature for 1 h. The solvent was removed from
the clear solution in vacuo, yielding a clear oil. Crystals
(m.p. 270–272 ◦ C) suitable for X-ray crystallography were
isolated from a dichloromethane–petroleum spirit (60–80 ◦ C)
solution of the compound. Intensity data were collected
at 293 K on a Bruker SMART Apex CCD diffractometer
for a block 0.08 × 0.10 × 0.25 mm3 . C50 H42 F6 O10 S2 Sn4 , M =
Copyright  2004 John Wiley & Sons, Ltd.
REFERENCES
1. Chandrasekhar V, Nagendran S, Gopal K, Steiner A, Zacchini S.
Chem. Commun. 2003; 862.
2. Orita A, Xiang J, Sakamoto K, Otera J. J. Organometal. Chem. 2001;
624: 287.
3. Davies AG. Organotin Chemistry. VCH: Weinheim, 1997.
Appl. Organometal. Chem. 2004; 18: 51–52
Документ
Категория
Без категории
Просмотров
2
Размер файла
83 Кб
Теги
tetraphenyl, report, ph2, crystallographic, dimeric, snosn, hydroxy, o3scf3, trifluoromethanesulfonatodistannoxane
1/--страниц
Пожаловаться на содержимое документа